Water → 4-Acetyl-n-(3-(1-acetylpiperazin-4-yl)phenyl)-2-nitroaniline

HRID 49816

반응식

HRID 49816 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7](F)=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1)=[O:3].[C:14]([N:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:24]=[C:25]([CH:27]=[CH:28][CH:29]=2)[NH2:26])[CH2:19][CH2:18]1)(=[O:16])[CH3:15].O>CN1C(=O)CCC1>[C:2]([C:4]1[CH:9]=[CH:8][C:7]([NH:26][C:25]2[CH:27]=[CH:28][CH:29]=[C:23]([N:20]3[CH2:19][CH2:18][N:17]([C:14](=[O:16])[CH3:15])[CH2:22][CH2:21]3)[CH:24]=2)=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1)(=[O:3])[CH3:1]

참가 물질

5

반응물 3

HCID 962WaterHCID 27346124'-Fluoro-3'-nitroacetophenoneHCID 111175391-[4-(3-Aminophenyl)piperazin-1-yl]ethan-1-one

생성물 1

HCID 223302264-Acetyl-n-(3-(1-acetylpiperazin-4-yl)phenyl)-2-nitroaniline

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
80 °C

실험 절차

A mixture of 1b (0.75 g, 4.1 mmol) and 2d (0.9 g, 4.1 mmol) in anhydrous NMP (2 ml) was heated to 80° C. overnight under a stream of nitrogen. After cooling water (20 ml) was added and the mixture was extracted with dichloromethane. The organic extract was dried over sodium sulfate and the solvent was removed under reduced pressure. The residue was purified by column-chromatography on silica gel using ethyl acetate as the eluent to yield 4-acetyl-N-(3-(1-acetylpiperazin-4-yl)phenyl)-2-nitroaniline as an oil.

후처리

  1. additionwas added
  2. extractionthe mixture was extracted with dichloromethane
  3. extractionThe organic extract
  4. dry with materialwas dried over sodium sulfate
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified by column-chromatography on silica gel

출처 및 근거

ORD 기록
ord-da6a3f7e113d4c7caef77cfec8bc0628
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710044B2

연결된 노트

불러오는 중…